CN101240382A - Method for preparing high dense TiAl-base alloy - Google Patents

Method for preparing high dense TiAl-base alloy Download PDF

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Publication number
CN101240382A
CN101240382A CNA2007100343834A CN200710034383A CN101240382A CN 101240382 A CN101240382 A CN 101240382A CN A2007100343834 A CNA2007100343834 A CN A2007100343834A CN 200710034383 A CN200710034383 A CN 200710034383A CN 101240382 A CN101240382 A CN 101240382A
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powder
sintering
pressing
base
presintering
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CNA2007100343834A
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Chinese (zh)
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CN100537802C (en
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刘咏
刘彬
张伟
何晓宇
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中南大学
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Abstract

The invention is a method for manufacturing high-density TiAl base alloy, which uses Ti powder, Al powder and other microelements powder as raw material. After the raw materials powder is uniformly mixed, cold pressure form by pressing or cold isostatic compaction, constrain presintering inside sintering mold, high-temperaturesintering and hot isostatic pressing. The raw materials are Ti powder, Al powder and other alloy elements powder, so the cost is low; compared with hot pressing and extrusion process, the process of the invention is simple, the devices are conventional devices, which effectively reduces cost; the TiAl alloy material for manufacturing has high density, the average density can reach up to 98% after hot isostatic pressing treatment; compared with other methods for manufacturing high-density TiAl base alloy with other elements powder, such as hot pressing, extrusion, etc., the size of blank of the TiAl base alloy manufactured by the invention is large (d>100mm), suitable for industrial production.

Description

A kind of method for preparing high dense TiAl-base alloy
Technical field
The present invention relates to a kind of preparation method of high dense TiAl-base alloy, belong to field of powder metallurgy.
Background technology
The castability of TiAl base alloy is relatively poor, easily produce the as cast condition defective, and powder metallurgy process has clear superiority at aspects such as eliminating macroscopical component segregation, loose, shrinkage cavity, the while powder metallurgy process prepares TiAl base alloy and also has homogeneous microstructure, tiny, can realize the newly net forming of product, thereby the difficulty that can avoid TiAl base alloy to be difficult to plastic making and mechanical workout reduces production costs and waits process characteristic, makes powder metallurgy process become a kind of important method for preparing the basic alloy of TiAl.Divide by starting material, utilize powder metallurgy process to prepare TiAl base alloy and can be divided into prealloy powder method and element powders method.Owing to fusing point height, the activity of Ti are big, the preparation of TiAl base alloy pre-alloyed powder needs strict CONTROL PROCESS, and with impurity such as minimizing oxygen, nitrogen, so price is very expensive.The element powders method adopts element ti, Al powder, do not need expensive prealloy powder and complicated processing unit, can effectively reduce production cost, simultaneously can also add various high molten alloy elements very easily, mix and pyroreaction by homogenizing, can effectively avoid component segregation, these all make the element powders method become a kind of very promising TiAl base alloy preparation technology.
Ti, Al element powders usually with the expansion significantly of volume, adopt the porosity of conventional vacuum sintering gained can arrive 30%~40% when TiAl base alloy is produced in reaction, even adopt the postorder hip treatment all to eliminate.Because the compactness extent of sintered metal product has decisive influence to its use properties, volumetric expansion is very unfavorable to follow-up processing and use.At present, the volumetric expansion significantly that produces during for restricted T i, the reaction of Al element powder, the technology that the metallurgical TiAl base of the high dense powder of multiple preparation alloy occurred is as heat pressing process, extruding and vacuum sintering, hot isostatic pressing process combined and Ceracon quasi-iso static pressing technology etc.Adopt heat pressing process can effectively suppress powder Ti, the Al expansion behavior in reaction process, and under the assistance of pressure, promote the densification behavior of Ti, Al element powders, thereby can effectively eliminate hole, obtain the material of high-compactness, the Liu Yong of Central South University etc. has been systematic research [Processing TiAl-Based alloy by Elemental Powder Metallurgy, Journal of MaterialsScience to the hot pressed sintering behavior of element ti, Al; Technology, 2000,16 (6), 605~610].Volumetric expansion effect when extruding and vacuum sintering, hot isostatic pressing process combined also can effectively reduce sintering obtains near fully dense TiAl base alloy [Wang G X, Dahms M.Synthesizing Gamma-TiAl Alloys by Reactive PowderProcessing.JOM, 1993 (5): 52~56], the purpose of extruding mainly is to destroy the oxide film of Ti, Al particle surface, by big extrusion ratio element ti, Al homogenizing on microcosmos area is more mixed simultaneously, thereby help the diffusion reaction of element ti, Al; Blank after the extruding is fibrous in the tissue topography that is parallel to the direction of extrusion, because the Al particle is extruded into fiber fines, the hole that stays after reaction is finished is very little, can effectively eliminate by vacuum sintering and follow-up hot isostatic pressing.But when this cold-pressing deformation method refinement Ti, Al constituent element size, must adopt the superelevation extrusion ratio, (extrusion ratio is 350), thereby this method is difficult to practical application industrial.In addition, someone also adopts Ceracon quasi-iso static pressing technology to obtain the TiAl base alloy [TaguchiK of high-compactness, Ayada M, et al.Near-net shape processing of TiAl intermetallic compounds ovapscudo HIP-SHS route.Intermetallics, 1995,3:91~98], in this technology when unidirectional stress is on ceramic particle, ceramic particle can evenly pass to pressure on the pressed compact as transmission medium, pressed compact is finished the densification behavior under the effect of three-dimensional stress (quasi-iso static pressing power).
More than a common ground of all multi-methods be exactly that technology is all comparatively complicated, cost is higher, is difficult to realize suitability for industrialized production.
Summary of the invention: the object of the present invention is to provide the technology of preparing of the metallurgical TiAl base of the cheap relatively high fine and close element powders of a kind of cost alloy, this technology adopts Ti powder, Al powder and other element powders directly to produce high fine and close TiAl base alloy material through low temperature control presintering+high temperature sintering.
A kind of method for preparing high dense TiAl-base alloy comprises:
1, be raw material with Ti powder, Al powder and other micro-powder, the constituent atoms proportioning is 50~60%Ti powder, 40~50%Al powder, 0~10% micro-powder; The particle diameter of Ti powder is 20~100 μ m, and the particle diameter of Al powder is 10~100 μ m, and trace element comprises Nb, Mn, C, Si, B, W, Y, Ce, TiB or TiB 2In one or several, the particle diameter of micro-powder is 20~100 μ m;
2. raw material powder carries out adopting mold pressing or isostatic cool pressing cold-press moulding to make the base of colding pressing after homogenizing is mixed, and pressure is 50~600Mpa during die forming, and pressure is 50~200Mpa during cold isostatic compaction;
3, the base of will colding pressing is put into constraint sintering mould, carries out vacuum and do not have the presintering of pressure and get the presintering base in vacuum sintering furnace, and vacuum tightness is 1 * 10 -1~10 -3Pa; The presintering system is: 200 ℃~250 ℃, and time 0.5~2h, 400 ℃~450 ℃, time 0.5~2h, 600 ℃~650 ℃, time 3~5h, 700 ℃~750 ℃, time 1~3h, each section temperature rise rate is 5 ℃/min, and top temperature is 800 ℃, and total treatment time is 5~12h;
4, remove constraint sintering mould after presintering is finished, the presintering base is carried out high temperature sintering again, high temperature sintering vacuum tightness is 1 * 10 -1~10 -3Pa is at 1200~1400 ℃ of insulation 1~3h, cold with stove;
5, the alloy billet behind high temperature sintering is carried out hot isostatic pressing to eliminate remaining hole, hot isostatic pressing carries out under Ar gas atmosphere, and pressure is 150~200Mpa, and temperature is 1200~1300 ℃, and the time is 3~5h.
The presintering process is carried out in constraint sintering mould, and constraint sintering mould is combined by gland, internal mold and adventitia; Internal mold is the type of the carving structure of the symmetric band tapering of two lobes, and conicity angles alpha (angle of inclined-plane and vertical direction) is 15 °~45 °; When pressed compact was put into internal mold, sandwiching a layer thickness between base substrate and mould inner wall was the molybdenum sheet interlayer of 1mm; Internal mold integral body is put into external mold, low pressure compacting on pressing machine then after gland is bumped into the internal mold opening end.
Raw material of the present invention is element ti powder, Al powder and other alloying element powder, and raw materials cost is low; Compare with hot pressing, extrusion process, technology of the present invention is simple, and equipment is conventional equipment, can effectively reduce cost; Though low temperature, high-temperature sintering process are to adopt pressureless sintering among the present invention, but the density height of the TiAl alloy material of its preparation, can reach more than 98% through average density after the hip treatment, this density than the TiAl base alloy of the pressureless sintering method preparation of routine is much higher, close with the density of the TiAl of prepared such as hot pressing, extruding base alloy, and the each several part porosity difference of blank is little; To prepare the method for high dense TiAl-base alloy compared with other element powders metallurgy, as hot pressing, extruding etc., big (the d>100mm), and the profile of blank can do suitable adjustment as required, is suitable for suitability for industrialized production of the size of the prepared TiAl of the present invention base alloy billet.
Description of drawings:
Fig. 1, process flow sheet of the present invention;
The structural representation of constraint sintering mould among Fig. 2, the present invention;
The process curve figure of control presintering process among Fig. 3, the present invention;
The TiAl base alloy material photomacrograph that Fig. 4, the present invention produce.
Embodiment
Embodiment 1: the employing granularity is that Ti powder and the granularity of 20~50 μ m is the Al powder of 20~50 μ m, carries out batch mixing by the composition proportion of Ti-50at.%Al; Die forming under the pressure of 200Mpa subsequently, making diameter is 120mm, the base of colding pressing of high 45mm; As Fig. 2, the base 4 of will colding pressing is put into constraint sintering internal mold 3, and pressed compact and interior intermode separate with molybdenum interlayer 2, then internal mold integral body are put into sintering external mold 5, on use gland 1 low pressure compacting on pressing machine.The constraint sintering mould that assembles is put into vacuum sintering furnace adopts process curve shown in Figure 3 to carry out vacuum presintering; Remove constraint sintering mould subsequently, the presintering blank is carried out the high-temperature vacuum sintering, sintering schedule is 1300 ℃, and 2h is cold with stove; Carry out hip treatment at last under Ar atmosphere, processing condition are 1250 ℃, 130Mpa, 4h.The TiAl alloy material that makes is of a size of d110mm * 35mm, and density is 97%.
Embodiment 2: the employing granularity is that Ti powder, the granularity of 20~50 μ m is the Al powder of 20~50 μ m and Nb powder and the W powder that granularity is 20~50 μ m, carries out batch mixing by the composition proportion of Ti-45Al-7Nb-0.4W (at.%); Die forming under the pressure of 200Mpa subsequently, making diameter is 120mm, the base of colding pressing of high 45mm; Pressed compact is put into constraint sintering mould, adopt process curve shown in Figure 3 to carry out vacuum presintering; Carry out vacuum high-temperature sintering subsequently, sintering schedule is: 1300 ℃, 2h is cold with stove; Carry out hip treatment at last, processing condition are 1250 ℃, 130Mpa, 4h; The fine and close base of TiAl base alloy that makes is of a size of d108mm * 34mm, and density is 97.5%.

Claims (4)

1. method for preparing high dense TiAl-base alloy is characterized in that: comprising:
(1) be raw material with Ti powder, Al powder and other micro-powder, the constituent atoms proportioning is 50~60%Ti powder, 40~50%Al powder, 0~10% micro-powder; The particle diameter of Ti powder is 20~100 μ m, and the particle diameter of Al powder is 10~100 μ m, and the particle diameter of micro-powder is 20~100 μ m;
(2) the material powder carries out adopting die forming to make the base of colding pressing after homogenizing is mixed, and pressure is 50~600Mpa during die forming;
(3) base of will colding pressing is put into constraint sintering mould, carries out vacuum and do not have the presintering of pressure and get the presintering base in vacuum sintering furnace, and vacuum tightness is 1 * 10 -1~10 -3Pa; The presintering system is: 200 ℃~250 ℃, and time 0.5~2h, 400 ℃~450 ℃, time 0.5~2h, 600 ℃~650 ℃, time 3~5h, 700 ℃~750 ℃, time 1~3h, each section temperature rise rate is 5 ℃/min, and top temperature is 800 ℃, and total treatment time is 5~12h;
(4) remove constraint sintering mould after presintering is finished, the presintering base is carried out high temperature sintering again, high temperature sintering vacuum tightness is 1 * 10 -1~10 -3Pa is at 1200~1400 ℃ of insulation 1~3h, cold with stove;
(5) alloy billet behind high temperature sintering is carried out hot isostatic pressing to eliminate remaining hole, hot isostatic pressing carries out under Ar gas atmosphere, and pressure is 150~200Mpa, and temperature is 1200~1300 ℃, and the time is 3~5h.
2. method according to claim 1 is characterized in that: described trace element comprises Nb, Mn, C, Si, B, W, Y, Ce, TiB or TiB 2In one or several.
3. method according to claim 1 is characterized in that: raw material powder carries out also can adopting the isostatic cool pressing cold-press moulding to make the base of colding pressing after homogenizing is mixed in the step (2), and pressure is 50~200Mpa during cold isostatic compaction.
4. a constraint sintering mould that is used for the described method of claim 1 is characterized in that: retrain the sintering mould and combined by gland, internal mold and adventitia; Internal mold is the type of the carving structure of the symmetric band tapering of two lobes, and conicity angles alpha is 15 °~45 °; When pressed compact was put into internal mold, sandwiching a layer thickness between base substrate and mould inner wall was the molybdenum sheet interlayer of 1mm.
CNB2007100343834A 2007-02-05 2007-02-05 A kind of method for preparing high dense TiAl-base alloy CN100537802C (en)

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CN101906548A (en) * 2010-07-09 2010-12-08 哈尔滨工业大学 Preparation method of TiB2 particle-reinforced TiAl-based composite material
CN101530916B (en) * 2009-04-15 2011-06-01 中南大学 Mold for controlling the defect of sintering expansion of powder metallurgy material
CN102126022A (en) * 2011-02-18 2011-07-20 中南大学 Constraint sintering die for controlling sintering deformation defect of powder metallurgical green body
CN102139370A (en) * 2011-01-14 2011-08-03 广州有色金属研究院 Method for preparing Ti2AlC self-lubricating and heat-resisting structural material
CN102416475A (en) * 2011-11-24 2012-04-18 西安瑞福莱钨钼有限公司 Method for preparing nuclear functional material tungsten-tantalum alloy plate
CN102528039A (en) * 2010-11-09 2012-07-04 德固萨有限责任公司 Method for the manufacture of a shaped body as well as green compact
CN102641890A (en) * 2012-04-28 2012-08-22 中南大学 Preparation method of powder metallurgy superfine crystal titanium aluminum base alloy panel
CN102660716A (en) * 2012-05-02 2012-09-12 哈尔滨工业大学 Preparation method of nanoparticle-reinforced Al-Fe-Cr-Ti-Re heat-resistant aluminum alloy sheet
CN102864320A (en) * 2012-09-24 2013-01-09 西北有色金属研究院 Preparation method of low-cost Ti-3Al-2V alloy
CN103122426A (en) * 2013-03-08 2013-05-29 山东金山汽配有限公司 Titanium-based powder metallurgy brake disc material and preparation method thereof
CN103143709A (en) * 2013-03-26 2013-06-12 哈尔滨工业大学 Method for manufacturing TiAl intermetallic compound component based on Ti elemental powder and Al elemental powder
CN104263981A (en) * 2014-09-17 2015-01-07 福建龙溪轴承(集团)股份有限公司 Method for preparing powder metallurgy titanium alloy bar
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CN101530916B (en) * 2009-04-15 2011-06-01 中南大学 Mold for controlling the defect of sintering expansion of powder metallurgy material
CN101906548B (en) * 2010-07-09 2012-06-06 哈尔滨工业大学 Preparation method of TiB2 particle-reinforced TiAl-based composite material
CN101906548A (en) * 2010-07-09 2010-12-08 哈尔滨工业大学 Preparation method of TiB2 particle-reinforced TiAl-based composite material
US9393088B2 (en) 2010-11-09 2016-07-19 Degudent Gmbh Method for the manufacture of a shaped body as well as a green compact
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CN102416475A (en) * 2011-11-24 2012-04-18 西安瑞福莱钨钼有限公司 Method for preparing nuclear functional material tungsten-tantalum alloy plate
CN102641890A (en) * 2012-04-28 2012-08-22 中南大学 Preparation method of powder metallurgy superfine crystal titanium aluminum base alloy panel
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CN107130160A (en) * 2017-05-24 2017-09-05 哈尔滨工业大学 A kind of Ti V Al base lightweight memorial alloys and preparation method thereof
CN107130139B (en) * 2017-06-15 2018-09-18 北京科技大学 A method of the addition intensified-sintered Powder Metallurgy TiAl based Alloys of Sn
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CN107119210A (en) * 2017-06-21 2017-09-01 苏州艾盾合金材料有限公司 A kind of extruder screw kneading block and its preparation technology
CN107699738A (en) * 2017-09-29 2018-02-16 成都露思特新材料科技有限公司 A kind of fine-grained TiAl alloy and preparation method thereof, aero-engine, automobile
CN109943790A (en) * 2017-12-20 2019-06-28 北京有色金属研究总院 The removing method of gas hole defect in a kind of injection forming said alloy
CN109628785B (en) * 2019-01-23 2020-04-21 宁波合盛新材料有限公司 Preparation method of 7XXX aluminum alloy billet
CN109628785A (en) * 2019-01-23 2019-04-16 宁波合盛专用车辆有限公司 A kind of preparation method of 7XXX aluminium alloy billet
CN109971996B (en) * 2019-04-10 2021-02-12 江苏宇豪新材料科技有限公司 TiB particle reinforced Ti-based composite material capable of effectively improving plasticity performance
CN109971996A (en) * 2019-04-10 2019-07-05 杨卫国 A kind of TiB particle enhancing Ti based composites that can effectively improve plastic property
CN110172606A (en) * 2019-06-11 2019-08-27 中山麓科睿材科技有限公司 A kind of preparation process of alumina dispersion-strenghtened copper compo pipe
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CN111215623A (en) * 2020-03-02 2020-06-02 北京理工大学 Powder metallurgy densification pressureless sintering method of Ti-Al alloy

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